Evolution of Microstructure and Exchange Bias
Characteristics of NiFe2O4/NiO nanocomposite
Department of Physics, North Orissa University, Takatpur, Baripada, Odisha, India.
Department of Physics, North Orissa University, Takatpur, Baripada, Odisha, India, pin-757003, Tel: +91 9437656274 ; Email:
Received: November 02, 2016; Accepted: November 10, 2016; Published: November 15, 2016
Mallick P (2016) Evolution of Microstructure and Exchange Bias Characteristics of NiFe2
/NiO nanocomposite. Nanosci
Technol 3(2): 1-7. DOI: 10.15226/2374-8141/3/2/00137
The occurrence of exchange bias (EB) characteristics in the
systems attracted research attention owing to their application
possibilities. This review highlights the effect of various parameters
on the evolution of microstructure and exchange bias characteristics
of NiFe2O4/NiO nanocomposite. The microstructure of NiFe2O4
present in NiFe2O4/NiO nanocomposite is strongly influenced by the
synthesis methods as well as the synthesis conditions. The influence
of various parameters like field cycle, molar ratio, size, temperature
etc. on the EB characteristics is discussed. For the occurrence of good
EB characteristics with promising application potentiality one need
to synthesize the system avoiding the formation of relatively larger
size NiFe2O4 particles or more ferromagnetic NiFe2O4 phase in the
Keywords: Nanocomposite, Exchange Bias, Inorganic compound,
Magnetic properties, NiFe2O4
In recent years, NiFe2O4 has attracted considerable research
attentions due to its diverse possible technological application
possibilities in microwave devices , magnetic drug delivery
, magnetic high-density data storage , catalysis [4, 5],
radio-frequency range , hyperthermia , gas sensing ,
humidity sensing  etc. The reduction of the size from bulk to
nanoscale optimizes the material properties regarding certain
technological purposes in many of these applications as new
phenomena arise due to enhancement of surface effect in the
nanoscale regime .The study of the properties of magnetic
nanoparticles is not only important from basic but also form
technological point of view [11, 12]. In addition, the transition
from single component to composite systems in the nanoscale
regime offers great possibilities for tailoring the performance
of the resultant composite . The magnetic nanocomposites
have attracted much attention in different fields due to their
synergistic effect and magnetic exchange interactions. These
nanocomposites opened up a new opportunity to develop the
excellent multifunctional materials with their excellent magnetic
Among the different well studied ferrite/metal oxide
nanocomposites, NiFe2O4/NiO system has attracted considerable
attention because of its excellent catalytic  and exchange bias
(EB) characteristics [16-23]. The existence of EB coupling in this
system demands its potentiality for designing permanent magnet
[24-26] as well as other various applications like data storage
(M-RAM), microelectronics (spin and tunneling valves), magnetic
sensors (read/write heads), and medicine (drug delivery) [27,
In this work, we review the effect of different conditions on
the microstructure and exchange bias characteristics of NiFe2O4/
There are several methods available in the literature for
the synthesis of NiFe2O4/NiO nanocomposite in power and
thin film form. Yanqing et al.,  synthesized NiFe2O4/NiO
by calcining the ball milled product of the initial ingredient of
NiO and Fe2O3. One can used chemical co-precipitation and
post thermal decomposition [16, 17, 20-23] to obtain NiFe2O4/
NiO nanocomposites. NiFe2O4/NiO nanocomposites have also
been synthesized by the thermal treatment of NiFe-layered
double hydroxides .NiO nanoparticles can be implanted into
NiFe2O4 nanowires chemically to prepare ordered NiO/NiFe2O4
nanocomposites . One can also adopt the Gen’s levitation jet
method to synthesize NiO/NiFe2O4 composite [30, 31]
NiFe2O4/NiO composite coating can be synthesized by heat
treating the electroplated Ni–Fe alloy . Thin films of NiFe2O4/
NiO were also synthesized using high-pressure microplasmabased
Among the different method, chemical co-precipitation and
post thermal decomposition method has been adopted in most
of the studies.
Evolution of Microstructure of NiFe2O4
The crystal structure of NiFe2O4 is not affected by varying the
synthesis conditions. However, the microstructure of NiFe2O4 is
strongly influenced by the synthesis conditions. For example:
(i) by changing the precursor or solvent in a similar procedure,
(ii) by changing the synthesis method using the same precursor.
Other parameters like sintering temperature, sintering time etc.
also play the crucial role in controlling the microstructure of
the NiFe2O4. The evolution of microstructure of NiFe2O4 under
different synthesis conditions are discussed in the followings.
Effect of Synthesis Method
Zhao et al.  synthesized NiFe2O4/NiO nanocomposite from
a nickel iron layered double hydroxide (NiFe-LDH) precursor
and by the chemical co-precipitation method. These authors
have seen that the calcination of NiFe-LDH precursor at 500 0C
led to the development of NiFe2O4 is ~ 6 nm in the NiFe2O4/NiO
nanocomposite. These authors also reported the formation of 20
nm size crystallite of NiFe2O4 by the calcination of the precursor
synthesized by the chemical co-precipitation method at 500 °C.
The crystallite size of the NiFe2O4 obtained by co-precipitation
method is about three times that of the material prepared using
the LDH precursor method. Ma et al.  synthesized NiFe2O4/
NiO composite by thermal oxidation of electroplated Ni–Fe alloy.
These authors have reported the formation of homogeneously
distributed dense and flat structure of NiFe2O4 in the matrix of
Pebley et al.  have synthesized nanostructured NiFe2O4 /
NiO films using high-pressure microplasma-based deposition by
varying Ni molar compositions (xNi). These authors reported that
the presence of both NiFe2O4 and NiO in the samples prepared
with xNi = 0.49−0.74. From the elemental mapping of Fe and Ni,
these authors suggested that 50−100 nm size NiFe2O4 crystals are
dispersed in a matrix of larger &tilde100−200 nm NiO grains.
It is clear from the above comparison that the size of NiFe2O4
is being influenced by changing the synthesis method.
Effect of Initial Precursor
It has been seen that the changing the initial precursor for
the synthesis in a particular synthesis procedure influences the
microstructure like crystallite size of the material. Even with
the same initial precursor with a slightly modification in the
synthesis condition also affect the crystallite size of the material.
Tian et al.  and He et al.  have synthesized NiFe2O4/NiO
nanocomposite by co-precipitation method using different initial
precursor and these authors have obtained different crystallite
size of NiFe2O4 (Table 1). Gong et al.  have used same initial
precursor and adopted same synthesis method as used by Tian
et al.  but due to slight modification in both their synthesis
condition led to the formation of different size NiFe2O4 (Table 1).
Effect of Calcination/Sintering Temperature and Time
Zhao et al.  also synthesized NiFe2O4/NiO nanocomposite
using NiFe-LDH precursor with Ni/Fe molar ratio ~ 3. These
authors calcined the NiFe-LDH precursor at 500 0C and seen
that the crystallite size of NiFe2O4 is ~ 6 nm. In an another work,
Zhang et al.  also synthesized NiFe2O4/NiO nanocomposite
NiFe–LDH precursor and obtained 44.73 nm size crystallites of
NiFe2O4 in NiFe2O4/NiO nanocomposite by calcined the NiFe–LDH
precursor (with a Ni/Fe molar ratio ~ 3) at 900 0C for 4 hours.
Tian et al. synthesised Ni1−xFexO (x = 0.09) by co-precipitation
method  and subjected the Fe doped NiO product to high
temperature sintering . These authors have studied the
effect of sintering temperature and time on the microstructural
property of the material . The evolution of crystallite size
of NiO and NiFe2O4nanoparticles with sintering temperature
is presented in Table 2. As indicated from the table (2) that
crystallites size of NiFe2O4 increases 0 to 55 nm with increasing
sintering temperature from 550 to 1000 0C (Figure. 1).Fitting
the variation of crystallite size ( D) of NiFe2O4with sintering
temperature (T ) to linear fit (Figure. 1) indicated that the size
of NiFe2O4increases linearly with the sintering temperature
following the relation:
The size of the crystallites of NiFe2O4 sintered at 600 0C also
shown to increase from 3 nm to 8 nm with increasing sintering
time from 1 to 3 hours (Table 2).
Effect of Molar Ratio
He et al.  synthesized Ni1 -xFexO (x = 0.15, 0.2, 0.3 and
0.5) bulk samples obtained using co-precipitation method
Table 1: NiFe2O4 nanoparticles with different size present in NiFe2O4/
NiO nanocomposite synthesized in a same method using different initial
Initial Precursor/ Sample
Size (nm) of NiFe2O4
NiCl·6H2O, FeCl3·6H2O, NH4HCO3
Tian et al. 
Ni(NO3)2.6H2O, Ni(NO3)3.9H2O, NH4HCO3
He et al. 
Gong et al. 
Table 2: Variation of crystallite size of NiO and NiFe2O4 present in Ni1−
xFexO (x = 0.09) sintered at different temperature [Reprinted from Tian
Z et al. J. Appl. Phys. 2014; 115(8): 083902 , with the permission of
Sintering Temperature (0C)
Sintering Time (h)
Crystallite Size of NiO (nm)
Crystallite Size of NiFe2O4 (nm)
and annealed at 650 0C for 12h in order to get NiFe2O4/NiO
nanocomposite. These authors have reported the formation of 20
nm size NiFe2O4 nanoparticles in NiFe2O4/NiO nanocomposite.
Gong et al.  have synthesized (100-x)NiO/(x)NiFe2O4
nanocomposites with x= 0, 2.5, 5, 8.3, 12.5, 25 were prepared
by a chemical co-precipitation method followed by sintering at
600 0C for 3h. They have reported that all the samples show an
average particle sizes of 12 nm with the formation of NiFe2O4/
NiO nanocomposite for x>2.5.
Evolution of Magnetic Properties of NiFe2O4
present in NiFe2O4/NiO
The occurrence of different types of magnetic ordering of
NiFe2O4 present in NiFe2O4/NiO is discussed in the followings.
He et al.  obtained NiFe2O4/NiO nanocomposite by
annealing Ni1 -xFexO (x = 0.15, 0.2, 0.3 and 0.5) synthesized by
co-precipitation method. Their temperature dependent of field
cooled magnetization measured at a field of 1 kOe indicated the
occurrence of ferromagnetic type magnetization in all samples.
Their study further indicated that the existence of the effective
exchange coupling interface between NiO and NiFe2O4. In another
work, Zhang et al.  also have reported the occurrence
of ferromagnetic behaviour in NiFe2O4/NiO nanocomposite
synthesized by using NiFe-LDH precursor.
Zhao et al.  reported the the occurrence of superparamagnetism
NiFe2O4/NiO nanocomposite synthesized by using NiFe-
LDH precursor and co-precipitation method. Their zero field cool
(ZFC) and field cool (FC) magnetization of the samples measured
at an applied field of 100 Oe indicated the sample prepared using
NiFe-LDH precursor having 6 nm size NiF2O4 nanoparticles
show the blocking temperature (TB) of 380 K whereas the TB is
~280 K for the sample prepared using co-precipitation method
having 20 nm size NiFe2O4nanoparticles. Their study indicated:
Figure 1:Variation of crystallite size of NiFe2O4in Ni1−xFexO (x = 0.09)
sintered at different temperaturefor 3 hours (Data taken from the ref.
). Line represents the linear fit to the data points.
(i) the occurrence of higher value of TB than the single phase Ni-
Fe2O4 nanoparticles with size < 10 nm [35, 36], (ii) the coupling
of NiO and NiFe2O4 could be a source of enhanced magnetization
stability as a result of which TB increased.
Spin glass Property
Tian et al. [16, 22] studied the effect of annealing on magnetic
behaviour of NiFe2O4 /NiO nanocomposite. Their magnetization
characterization indicated that the saturation magnetization of
all the samples increase with increasing annealing temperature.
The coercivity on the other hand follows a nonmonotonic size
dependencies and show the maximum value for the sample with
15 nm size NiFe2O4 nanoparticles.These authors pointed out
that the nonmonotonic behaviour of coercivity could be due to
the variation of total anisotropy arise from the contribution of
NiFe2O4 cores and the interfacial exchange coupling energy [37,
38]. Their ZFC and FC magnetization indicated that the ZFC and FC
magnetization curves diverge below certain temperature called
irreversibility temperature. The divergences become smaller
with increasing the size of NiFe2O4 nanoparticles and both the
curve fully coincides for sample with size of NiFe2O4 nanoparticles
is above 32 nm. These authors also have seen that the peak of ZFC
magnetization curves shifts to lower temperatures, correlated
with the reduction of magnetic disorder at interfaces .
In order to understand the low temperature magnetic
behaviour of the samples, these authors , undertaken
temperature dependent ZFC and FC magnetization at various
magnetic fieldfor sample with 8 nm size NiFe2O4 nanoparticles.
Their study indicated that the occurrence of spinglass phase due
to the existence of intermediate structural disordered layers at
NiFe2O4/Ni1-xFexO interfaces [16, 22].
Exchange bias (EB) effect in NiFe2O4/NiO
In 1956, the phenomenon of exchange bias (EB) was
discovered by Meiklejohn and Bean  in ferromagnetic (FM)
Co particles coated antiferromagnetic (AFM) CoO which referred
to the shift of a hysteresis loop along the magnetic field axis.In
order to generate EB effect, there must be the co-existence of
two phases i.e. one with net magnetic moment whose magnetic
moment can be reversed and other phase which can exert a
torque action on the spins of the former during the process of
magnetization reversal [22, 28, 40]. Since its discovery, EB
effect has also been studied in other systems like ferrimagnetic
(FiM) coupled with other (AFM or FM) [41, 42] or spinglass (SG)
coupled with other (FM, AFM orFiM) [28, 43, 44]. In recent years,
EB in nanoparticle systems has attracted much attention because
of the unique properties of nanoparticles and their potential
technological applications .In contrast to bilayer systems,
the inclusion of FM cluster in AFM matrix is interesting from
fundamental point of view .
The phenomenon of EB in the system is quantified by
calculating EB field, HEB
and the coercivity,
are the left and right coercive field, respectively [46, 47]. The vertical magnetization shift
is also calculated by taking the difference of saturation magnetization between the measured hysteresis loop and the loopcentered in the M axis .
In this section, we discuss the EB effect of NiFe2
nanoparticles embedded in NiO matrix. There are several effects like field cycle, molar ratio, size, temperature etc. which affects the EB in the system are discussed in the followings.
Effect of Cooling Field
Tian et al. studied the effect of cooling field on the EB characteristics of NiFe2
nanoparticles embedded in NiO matrix . Their study indicated that the
increases with increasing cooling field from 0 to 12 kOe and the same saturates thereafter. These authors argued that only a part of spins at the Ferri/AFM interface are pinned along the cooling field direction for smaller fields and more spins are pinned along the field direction which causes the enhancement of exchange interaction with increasing cooling field. As a result of which
increases with increasing cooling field. For higher cooling field (>12 kOe), the pinned spins along the field saturates which resulted into the saturation of
Effect of Field Cycle
Tian et al.  studied the effect of field cycle on the EB characteristics of NiFe2
nanoparticles embedded in NiO matrix. Their study indicated that both
decrease with the increasing field cycling .
Effect of Cycle Dependent Cooling Field
In another work, Tian et al. studied the effect of cycle dependent cooling field on the EB characteristics of NiFe2
nanoparticles embedded in NiO matrix . Their study indicated that the HEB increases with increasing cooling field for a particular cycle and the relative change in HEB i.e.
decreased by ~ 71% from its initial value for cooling field at 0Oe whereas the same decreased by 54% for cooling field at 40 kOewith increasing loop cycle to = 9 . These authors argued that decrease of HEBwith increasing loop cycle reflects the configurationalrearrangements of the spin structure and can be expressed by the following discretized Landau-Khalatnikov equation [48, 49]:
are fitting parameters which describe
in the limit of infinite loops and the characteristic decay rate of the training behavior, respectively. The monotonic decrease of
with increasing cooling filed in case of Tian et al.  also confirm the reduction of trainingeffect for high cooling field. The authors assumed the coexistence of the two possible mechanism on training effect  to their case i.e. (i) FM magnetization is in a multi-domain state for
=0 Oe, which reverses via a symmetric mechanism, and can lead to the suppression of training effect, (ii) higher field cooling results in a single-domain state, asymmetric reversal process via domain wall and nucleation process take place which led to larger training effect.
Effect of Size Dependent Field Cycle
In order to see the size dependent field cycle effect on EB characteristics, Tian et al. studied the variation of normalized
and normalized coercivity enhancement
as a function of different size of NiFe2
nanoparticles embedded in NiO matrix. Their result indicated that both the parameter decrease with increasing size of NiFe2
with a minima for the sample with 22 nm size NiFe2
nanoparticles. The suppression of normalized
by 75% and 82% respectively for the sample with 22 nm size NiFe2
nanoparticles indicated the correlation between
as seen for other systems [51, 52]. The reduction in
could be due to the weakening of interfacial exchange coupling energy due to the depinning of frozen AFM spins and the loss of interfacial coupling energy between FM/AFM system after each field cycle. Further, the slower change in
for larger particle size could be due to enhancement of the interfacial coupling stiffness for larger AFM particles which leads to relatively smaller interfacial energy losses after each field cycle .
Effect of Molar Ratio
Effect of NiFe2O4 ratio
Gong et al.  synthesized (100-x)NiO/(x)NiFe2
nanocomposites by varying x(x= 0, 2.5, 5, 8.3, 12.5, 25) by a chemical coprecipitation method. These authors pointed out that NiFe2
has not beendetected by XRD for the composite sample with x=2.5. For x concentration > 2.5, both antiferromagneticNiO and ferrimagnetic NiFe2
coexist in the nanocomposites. These authors calculated the average particle size as 12 nm for all the samples from XRD line width using Scherrer formula  which agree with their TEM observation.Their study indicated that the
for pure NiO (i.e. with x=0) is 1.1 kOe which increases with increasing x concentration i.e. concentration of NiFe2
up to x = 2.5 and the same decreases with further increasing x concentration.The observation of
for pure NiO is attributed to the exchange coupling between the spins of the AFM core and the uncompensated surface moments of NiO nanoparticles [54-56]. The large loop shift and coercivity observed in AFM nanoparticles is a consequence of the transition from two-sublattice to multisublattice of the AFM NiO nanoparticles [44, 57]. It has been reported that the
decrease with increasing temperature in AFM/FM or AFM/FI systems because the excess thermal energy decreases the exchange coupling between AFM/FM and AFM/FI . The strong interfacial exchange coupling between NiO and NiFe2
is the cause for the increase of
with increasing NiFe2
concentration up to x = 2.5 . Hence, the authors suggested that nanocomposite with x=0.25 is the percolation threshold of the nanocomposites which further confirms the observation of He et al.  that the presence of more NiFe2
phase in NiO or the formation of isolated NiFe2
in the composite for x>2.5 reduces the interface coupling between NiO and NiFe2
as a result of which
decreases in the samples. Similar type of behaviour has also been reported for Ni/NiO  and NiFe2
/NiO  nanocomposites.
Effect of Fe concentration in Ni1-xFexO
He et al.  synthesized Ni1-x
O with different Fe concentration by co-precipitation method and finally annealed the samples at 6500C for 12 hours. In order to study the effect of Fe concentration of the EB characteristics of the samples, the authors calculated
as a function of temperature for the samples with different Fe concentrations from M-H curve of the samples taken by cooling the sample at an applied field of 1kOe from 300K. These authors reported that the value of
decreases with increasing the Fe content x at the same temperature. These authors argued that the enhancement of ferromagnetic type interactions among NiFe2
particles with increasing Fe content could be the cause of suppression of
Effect of Ni/Femolar ratios
Zhao et al.  synthesized different NiFe2
/NiO nanocomposites by calciningNiFe-LDH precursors with different NiII/FeIIImolar ratios at 500 0C. These authors have seen that the value of
increased from 53.6 Oe to 330.4 Oe with increasing NiII/FeIII molar ratios from 2:1 to 4:1. This study further confirms the suppression of
with increasing size or fraction of NiFe2
phase in NiFe2
/NiO as was seen by He et al. .
In another work, Pebley et al.,  synthesized NiFe2
/NiO nanocomposites by varying Ni molar fraction and studied the EB characteristics of the samples with Ni molar fraction.These authors reported that both
under FC condition increase with increasing Ni molar fraction in the sample. This is in accordance with the previous observations that the interfacial density between the NiFe2
and NiO phases increases with increasing Ni content.
Effect of Sintering Temperature
In order to understand the suppression of
with increasing Fe content [see section 5.3.2], He et al.  also undertaken the effect of sintering temperature which resulted into larger size NiFe2
particles in NiFe2
/NiO with increasing sintering temperature. Their study indicated that the
of the sample decreases with increasing sintering temperature and the
nearly vanishes for the sample sintered at 850 0C for 12 hours. With increasing sintering temperature, the size of particles become larger and the NiFe2
particles may form ferromagnetic type clusters in NiO matrix as result of which effective coupling among the NiFe2
and NiO decreases. Similar types of observations have also been reported [19, 33, 60-62]. Hence it is clear from the study that relatively larger size NiFe2
particles or more ferromagnetic NiFe2
phase in the system is not the good choice for the occurrence of EB in this system.
In another work, Tian et al.  sintered their sample at various temperatures to investigate the NiFe2
/NiO. The authors have seen that the size of NiFe2
increasedfrom 0 to 55 nm with increasing sintering temperature from 550 to 1000 0C (Figure. 3).The authors also sintered the same sample at 6000C for 1 hour to get the sample with ~ 3 nm size NiFe2
particles. Their study of temperature dependent
indicated that the EB field decreases with increasing temperature and vanishes above 250 K for all samples (i.e. irrespective of crystallite size of NiFe2
and the same decreases rapidly for the sample with smaller size (12 nm) NiFe2
.The variation of
with temperature is in agreement with the variation of
for smaller size NiFe2
particles. However, no similar variation in both the parameters are shown for samples with size NiFe2
particles > 22 nm. In order to understand this behaviour, the authors plotted
for samples with different size of NiFe2
particles. Their results indicated that the existence of linear relationship between
for the samples with size of NiFe2
particles 8 nm indicated the correlation among them. The existence of linear dependency hence EB could be due to the coupling between the ferrimagnetic phase and the spin glass like phase formed due to structural disorder at the interface. The authors also pointed out that the open and unsaturation of field cooled loop measured at 10 K for sample with 8 nm size NiFe2
 further confirms the existence of spin glass like phase [60, 63]. The linear relationship between
deviates for the sample with size of NiFe2
particles is ~ 12 nm and the same show two linear dependency for the sample with size of NiFe2
particles is ~ 22 nm. These authors  stated that the deviation of linear dependency could be due to coexistence of two interfacial exchange coupling: one is the exchange coupling between ferromagnetic NiFe2
core and the spinglass like layer related to the structural disorder region in Ni1-x
O nanoparticles and the other arise from the coupling of the NiFe2
phase and antiferromagnetic NiO phases.
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